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JP5199875B2 - How the bubble column reactor works - Google Patents
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JP5199875B2 - How the bubble column reactor works - Google Patents

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JP5199875B2
JP5199875B2 JP2008535912A JP2008535912A JP5199875B2 JP 5199875 B2 JP5199875 B2 JP 5199875B2 JP 2008535912 A JP2008535912 A JP 2008535912A JP 2008535912 A JP2008535912 A JP 2008535912A JP 5199875 B2 JP5199875 B2 JP 5199875B2
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column reactor
flushing medium
flushing
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bubble column
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シュナイダー，リヒャルト
エム フリッツ，ペーター
ムッシェルクナウツ，ゼバスティアン
ベルト，ハインツ
アリ，タラル
モウサ，フアド
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C7/00—Purification; Separation; Use of additives
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/005—Separating solid material from the gas/liquid stream
    • B01J8/006—Separating solid material from the gas/liquid stream by filtration
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C2/00—Preparation of hydrocarbons from hydrocarbons containing a smaller number of carbon atoms
    • C07C2/02—Preparation of hydrocarbons from hydrocarbons containing a smaller number of carbon atoms by addition between unsaturated hydrocarbons
    • C07C2/04—Preparation of hydrocarbons from hydrocarbons containing a smaller number of carbon atoms by addition between unsaturated hydrocarbons by oligomerisation of well-defined unsaturated hydrocarbons without ring formation
    • C07C2/06—Preparation of hydrocarbons from hydrocarbons containing a smaller number of carbon atoms by addition between unsaturated hydrocarbons by oligomerisation of well-defined unsaturated hydrocarbons without ring formation of alkenes, i.e. acyclic hydrocarbons having only one carbon-to-carbon double bond
    • C07C2/08—Catalytic processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00008—Controlling the process
    • B01J2208/00539—Pressure
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F110/00—Homopolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
    • C08F110/02—Ethene

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Description

本発明は、カラム反応器を備えた気泡塔反応器の動作方法であって、カラム反応器が、カラム反応器を頂部反応区画および底部区画に分割するスパージャープレート(sparger plate)を有するものである気泡塔反応器の動作方法に関する。 The present invention provides a method of operating a bubble column reactor equipped with a column reactor, a column reactor, those having a sparger plate (sparger plate) for dividing the column reactor at the top reaction zone and the bottom section It relates to a method of operating a bubble column reactor.

気泡塔反応器が当該技術分野において広く知られている。気泡塔反応器は、例えば、エチレンをオリゴマー化して線状アルファ・オレフィン（ＬＡＯ）を形成するために利用される。そのような気泡塔反応器は、スパージャープレートにより上側反応区画および底部区画に分割されるカラム反応器を備えている。モノマーのガス状供給物が底部区画を介してカラム反応器中に導入され、スパージャープレートを通過し、上側区画においてモノマー、溶媒および触媒を含む均質溶液となり、次いで、線状アルファ・オレフィンを形成する。上側反応区画の頂部から、ガス状生成物などが除去される。さらに、溶媒、触媒、溶解したモノマーおよび線状アルファ・オレフィンを含む液体混合物を除去するためのラインが設けられている。 Bubble column reactors are widely known in the art. Bubble column reactors are utilized, for example, to oligomerize ethylene to form linear alpha olefins (LAO). Such bubble column reactors comprise a column reactor that is divided into an upper reaction section and a bottom section by a sparger plate . A gaseous feed of monomer is introduced into the column reactor via the bottom compartment, passes through the sparger plate and becomes a homogeneous solution containing monomer, solvent and catalyst in the upper compartment and then forms linear alpha olefins. To do. Gaseous products and the like are removed from the top of the upper reaction zone. In addition, a line is provided for removing a liquid mixture comprising solvent, catalyst, dissolved monomer and linear alpha olefin.

従来の気泡塔反応器において、スパージャープレートから滴り(weeping)が生じ、これが底部区画の詰まりの原因になるという問題がある。このことはしばしば、潜在的な機械的損傷が生じ、スパージャープレートの上のガス分布が乱れ、スパージャープレートの下の反応性材料による底部区画と出口ラインの詰まりが生じるかもしれないという欠点を持つことになる。 In conventional bubble column reactors, there is a problem that weeping occurs from the sparger plate , which causes clogging of the bottom compartment. This often has the disadvantage that potential mechanical damage may occur, gas distribution over the sparger plate may be disturbed, and the bottom compartment and outlet line may be clogged by reactive material under the sparger plate. Will have.

したがって、本発明の課題は、従来技術の欠点を克服した気泡塔反応器およびその動作方法を提供することにある。特に、気泡塔反応器中のスパージャープレートの滴りの発生が避けられるまたは少なくとも制御されるという気泡塔反応器および方法を提供すべきである。 Accordingly, it is an object of the present invention to provide a bubble column reactor that overcomes the disadvantages of the prior art and a method of operating the same. In particular, a bubble column reactor and method should be provided in which sparging of sparger plates in the bubble column reactor is avoided or at least controlled.

この課題は、フラッシング媒質を導入し廃棄するための入口ラインと出口ラインが底部区画に連結されることにより達成される。   This object is achieved by connecting an inlet line and an outlet line for introducing and discarding the flushing medium to the bottom compartment.

出口ラインは、カラム反応器の下流のパイプまたは設備に連結されることが好ましい。   The outlet line is preferably connected to a pipe or facility downstream of the column reactor.

ある実施の形態において、フラッシング媒質は、線状アルファ・オレフィンおよび芳香族類からなる群より選択される。   In certain embodiments, the flushing medium is selected from the group consisting of linear alpha olefins and aromatics.

前記課題はさらに、カラム反応器を頂部反応区画および底部区画に分割するスパージャープレートを有するカラム反応器を備えた気泡塔反応器を動作する方法であって、フラッシング媒質を、底部区画に、それぞれ、入口ラインおよび出口ラインを介して、導入し、そこから廃棄する方法により達成される。 The subject is further a method of operating a bubble column reactor with a column reactor having a sparger plate that divides the column reactor into a top reaction section and a bottom section, wherein a flushing medium is applied to the bottom section, respectively. This is achieved by a method of introducing and discarding through the inlet and outlet lines.

フラッシング媒質を、出口ラインから、カラム反応器の下流のパイプまたは設備に移送することが好ましい。   It is preferred to transfer the flushing medium from the outlet line to a pipe or facility downstream of the column reactor.

モノマーのガス状供給物を底部区画中に導入することがさらに好ましい。   More preferably, a gaseous feed of monomer is introduced into the bottom compartment.

最後に、最も好ましい実施の形態において、底部区画は連続的にフラッシングされる。   Finally, in the most preferred embodiment, the bottom compartment is continuously flushed.

意外なことに、従来の気泡塔反応器の欠点は、カラム反応器の底部区画を、好ましくは連続的に、フラッシング媒質でフラッシングすることによって、克服されることが分かった。底部区画をフラッシングすることによって、反応性または非反応性の材料（スパージャープレートの滴りにより生じる）は、底部区画から廃棄される。フラッシングに使用された媒質は、カラム反応器の下流に位置するパイプまたは設備に移送されることが好ましい。本発明の気泡塔反応器に、フラッシング媒質の底部区画を出入りする流入速度と流出速度を制御し、またスパージャープレートの上でカラム反応器を去る出口流の排出速度も制御することが好ましい制御ユニットが設けられることがさらに好ましい。 Surprisingly, it has been found that the disadvantages of conventional bubble column reactors are overcome by flushing the bottom section of the column reactor, preferably continuously, with a flushing medium. By flushing the bottom compartment, reactive or non-reactive material (caused by sparger plate drips) is discarded from the bottom compartment. The medium used for flushing is preferably transferred to a pipe or facility located downstream of the column reactor. In the bubble column reactor of the present invention, it is preferable to control the inflow rate and the outflow rate of entering and exiting the bottom section of the flushing medium, and also controlling the discharge rate of the exit stream leaving the column reactor on the sparger plate. More preferably, a unit is provided.

本発明の気泡塔反応器およびその動作方法の追加の利点および特徴を、添付の図面を参照してさらに説明する。   Additional advantages and features of the bubble column reactor of the present invention and method of operation thereof will be further described with reference to the accompanying drawings.

図１によれば、カラム反応器１を頂部反応区画３および底部区画４に分割するスパージャープレート２を有する本発明の気泡塔反応器が示されている。頂部反応区画３には、溶媒、モノマー、触媒および既に調製された線状アルファ・オレフィンを含む均質混合物が少なくとも部分的に充填されているのが分かる。溶媒、モノマーおよびガス状線状アルファ・オレフィンを含むガス状成分がライン５を介して、さらなる処理のために頂部反応区画３から除去される。さらに、バルブ７を有するライン６が、さらなる処理のために、溶媒、溶解したモノマー、触媒および液体線状アルファ・オレフィンを含む液体混合物をカラム反応器１から除去するために設けられている。 Referring to FIG. 1, a bubble column reactor of the present invention is shown having a sparger plate 2 that divides a column reactor 1 into a top reaction section 3 and a bottom section 4. It can be seen that the top reaction zone 3 is at least partially filled with a homogeneous mixture comprising solvent, monomer, catalyst and linear alpha olefin already prepared. Gaseous components including solvent, monomer and gaseous linear alpha olefin are removed from the top reaction zone 3 via line 5 for further processing. In addition, a line 6 having a valve 7 is provided to remove from the column reactor 1 a liquid mixture comprising solvent, dissolved monomer, catalyst and liquid linear alpha olefin for further processing.

モノマーのガス状供給物は、供給ライン８を介して底部区画４に導入され、１つ以上のノズル９などを介して散布される。次いで、分配されたガス状供給物がスパージャープレート２に通過せしめられ、頂部反応区画において均質混合物に散布される。 A gaseous feed of monomer is introduced into the bottom section 4 via a supply line 8 and is sprayed via one or more nozzles 9 and the like. The distributed gaseous feed is then passed through the sparger plate 2 and sprinkled into the homogeneous mixture in the top reaction zone.

カラム反応器１はさらに、フラッシング媒質を底部区画４に導入するための入口ライン１０も備えている。このフラッシング媒質は、バルブ１２を持つ出口ライン１１を介して底部区画４から廃棄される。出口ライン１１は、図１に示された実施の形態によれば、さらに処理されるように、カラム反応器１の下流のさらに別のパイプまたは設備に連結されている。 The column reactor 1 further comprises an inlet line 10 for introducing a flushing medium into the bottom compartment 4. This flushing medium is discarded from the bottom section 4 via an outlet line 11 with a valve 12. Outlet la Lee down 11, according to the embodiment shown in FIG. 1, as will be further processed, is connected to a further pipe or equipment downstream of the column reactor 1.

底部区画４に出入りするフラッシング媒質の流入速度および流出速度を制御し、バルブ７および図示されていない他の設備を制御するための制御ユニット（図示せず）も設けられていてよい。   A control unit (not shown) for controlling the inflow and outflow rates of the flushing medium entering and exiting the bottom compartment 4 and for controlling the valve 7 and other equipment not shown may also be provided.

底部区画がフラッシング媒質により連続的にフラッシングされることが好ましい。フラッシング媒質が、底部区画の実質的に全体に渡り撒き散らされて、徹底的かつ十分なフラッシングが行われることがさらに好ましい。   It is preferred that the bottom compartment is continuously flushed with a flushing medium. More preferably, the flushing medium is scattered over substantially the entire bottom section to provide thorough and sufficient flushing.

本発明の気泡塔反応器またはその動作方法では、スパージャープレートの滴りは避けられないであろうが、潜在的な機械的損傷、スパージャープレート上の気体分布の乱れ、およびスパージャープレートの下の材料による底部区画と出口ラインの詰まりなどの、それに関連する結果は克服されるであろう。 The bubble column reactor or a method of operation of the present invention, under but would inevitably drips sparger plate, potential mechanical damage, the gas distribution on the sparger plate turbulence, and sparger plate The associated results, such as clogging of the bottom compartment and outlet line with the material, will be overcome.

先の説明、特許請求の範囲および図面に開示された特徴は、別々とその任意の組合せの両方で、本発明をその多種多様な形態で実施するための素材である。   The features disclosed in the foregoing description, claims and drawings are materials for carrying out the invention in its various forms both separately and in any combination.

本発明の気泡塔反応器の概略図Schematic of the bubble column reactor of the present invention

１ カラム反応器
２ スパージャープレート
３ 頂部反応区画
４ 底部区画
９ ノズル 1 column reactor 2 sparger plate 3 top reaction section 4 bottom section 9 nozzle

Claims (5)

線状アルファオレフィンを形成するためのエチレンのオリゴマー化において、カラム反応器を備え、該カラム反応器を頂部反応区画および底部区画に分割する（i）スパージャープレート、（ii）入口ライン、（iii）出口ラインおよび（iv）供給ラインが該底部区画に連結された、前記エチレンのオリゴマー化を行うための気泡塔反応器を動作させる方法であって、
モノマーのガス状供給物を前記供給ラインを介して前記底部区画に供給するとともに、フラッシング媒質を前記入口ラインを介して前記底部区画に導入して該底部区画をフラッシングし、その後、前記出口ラインを介して前記底部区画からフラッシング媒質を排出することにより、前記底部区画から反応性または非反応性の材料を廃棄することを特徴とする方法。In ethylene oligomerization to form linear alpha olefins, a column reactor is provided that divides the column reactor into a top reaction section and a bottom section (i) a sparger plate , (ii) an inlet line , (iii ) A) operating a bubble column reactor for the oligomerization of ethylene, wherein an outlet line and (iv) a feed line are connected to the bottom section,
Supplies the gaseous feed monomer to the bottom compartment through the supply line, and flushing the bottom side section by introducing a flushing medium into the bottom ku image through the inlet line, then the outlet line how by discharging the bottom ku picture or al flushing medium, and discards the reactive or non-reactive materials from the bottom compartment through the. 前記フラッシング媒質を、前記出口ラインから前記カラム反応器の下流のパイプまたは設備に移送することを特徴とする請求項１記載の方法。Wherein the flushing medium, The method of claim 1, wherein the transferring to the downstream pipe or equipment of the outlet line or al the column reactor. 前記底部区画を連続的にフラッシングすることを特徴とする請求項１または２いずれか１項記載の方法。Claim 1 or 2. Method according to any one characterized by continuously flushing the bottom ku picture. 前記フラッシング媒質が、前記線状アルファ・オレフィンおよび芳香族類からなる群より選択されることを特徴とする請求項１から３いずれか１項記載の方法。4. A method according to any one of claims 1 to 3 , wherein the flushing medium is selected from the group consisting of the linear alpha olefins and aromatics. 前記フラッシング媒質の流入速度および流出速度を制御ユニットが制御することを特徴とする請求項１から４いずれか１項記載の方法。The method of claims 1 4, wherein any one of the inflow velocity and outflow speed control unit, characterized in that the control of the flushing medium.
JP2008535912A 2005-10-20 2006-09-06 How the bubble column reactor works Active JP5199875B2 (en)

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EP05022865A EP1777209A1 (en) 2005-10-20 2005-10-20 Method for oligomerization of ethylene and reactor system therefor with removal of heavy molecular weight oligomers
PCT/EP2006/008652 WO2007045306A1 (en) 2005-10-20 2006-09-06 Method for oligomerization of ethylene and reactor system therefor with removal of heavy molecular weight oligomers

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CN101291892A (en) 2008-10-22
WO2007045306A1 (en) 2007-04-26
US20090214405A1 (en) 2009-08-27
CN101291726A (en) 2008-10-22
US8058369B2 (en) 2011-11-15
JP2009511721A (en) 2009-03-19
EP1777209A1 (en) 2007-04-25
WO2007045305A1 (en) 2007-04-26
MY148940A (en) 2013-06-14
RU2008119814A (en) 2009-11-27
JP2009511267A (en) 2009-03-19

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